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Martedì, 02 Aprile 2019 14:27

Heating the Substance Again. Distillation Circulation Coobation

The distillation has something magical, we can’t figure out why a substance gets refined through heat and the passing in another container, or even circulating, which is rising and falling in the same glass balloon.

We just know it works: through this process the substances lose some of their toxicity, become more digestible or refined, more alcoholic, more penetrating or concentrated.

Moreover, through distillation or movement, we can literally change the nature of some particular substances. This happens in particular when we put them through a specific degree of heat, under vacuum, or eventually when, during distillation, we use special devices; or if we add other reagents able to cement the substance or catalyze the process, in some cases functioning as a fire themselves.

The mystery of the shaping fire involves everything, every phenomena, the living ones as well. So there are several fires in our world, that give shape to the embryo, flavor and texture to the wine, a form to the trees, to the leaves, in a continuous process that never begins and never ends.

We can see through this mystery and appreciate the knowledge that comes therein, but only if we are able to consider this world as a whole living entity, not just some/thing separate from us.

Antique instruments for the eternal art/science

Once we understand the articulated simplicity of antique instruments, we will also fully understand how the modern and contemporary ones work, what expect from them and how regulate, change or contradict the standard use of them.

Let’s examine the general issues related to the transition from a balloon to a receiver.

  • We need to produce the passage of the liquid into its gaseous form, from the distiller balloon to the receiver.
  • The substances are of a different nature, being oily, alcoholic, thick or thin, liquid or with more phlegm, therefore their passage through the instruments could be more or less easy.
  • We rather need only a part of the substance, leaving the other in the balloon or in the receiver to be used differently, to be thrown or to be disposed of.
  • We need or prefer an easier and faster passage of the distillate therefore cooling it up.
  • Or we strive to obtain our distillation with the lowest heat possible.
  • We require a sublimation in the distillation, that is the transition of the substance from liquid and vapour to solid and crystallised.
  • When the substance to be distilled is solid or the form of its passage is vapour, or thinner still, air or gas and the latter should be channeled through.
  • And then eventually pushed to solidify or crystallise through cold temperature.
  • Then there is the variable of coobation and the consequent need to easy get to the caput, remove and grind it to receive again the distilled liquid.

Considering what is described above, and more besides, there is in the alchemical tradition a fair amount of labware and three different traditional directions of distillation as it is outlined below:

Three different Directions in Ancient Distillation

Distillation_2

1) For ascenso (by elevation), In general It needs cooling...

distillation_3

2) For the side

distillation_4

3) For descenso (by descending). It has a guide or some glass shape that leads the vapours to drip into the rostrum. This kind of shape like a pocket is present also in the oldest heads made appositely for precise phials.

Parts of an Ancient system of Distillation

distillation_6

Diagram of the insertion phial head

distillation_7
  • A - head, or helm[1]
  • B - ursale (flask with large neck and opening) but here you could put also a vesica, a phial or a cucurbit
  • C - chapel (large skillet = Arabic: Al Tannur i.e. athanor) with coarse sand (sand bath); it is often called "athanor" an blind alembic, a crucible, or a vase/egg (closed towards the end of certain works) or more often the whole of the coal furnace, a multifunctional tower that holds the plan for the covered crucible, down near the coal and higher up various chapels with flasks, et cetera
  • D - rostrum, nose or beak possibly with coolant G
  • A + D = alembic
  • E - receptacle that receives = receiver
  • F - source of heat: in ancient times it was coal of various origins, enclosed in a multifunctional tower, in the nineteen century it was coke coal "American" producing as little smoke as possible, then butane / propane and finally the electricity that, almost always, is the best form of heat: the safest form of heati and the easiest to adjust
  • G - coolant
  • K - normal neck of a bowl to insert more easily in a helm
  • K1 - wide neck of ursale to retrieve more easily the kaput
  • K2 - the longer neck of the so called "phials"
  • K3 - very long neck to circulate better, or to force the vapours to rise more

The single parts of a distillation apparatus

In the past centuries clay, porcelain, stoneware, tin-plated copper and, in some cases, common glass were used: with the ever-present danger that a single drop of cold water on the hot piece of pottery or glass could crack them and stop the whole process.

The Lute. In fact there were a large amount formulas of lute, or lutum[2], substances used not only to close more precisely the joints, but also all those breaks and cracks inevitable in those days: even hardened paper was pasted on the stoneware, clay or glass ware, or strips of animal intestines tied on and then glued with ingenious mixtures.

The glass used in the laboratory were the same as the ones in the windows, but they were thicker, and blown with more expertise: then with the addition of boron and of silicon and, furthermore, with the fusion of the pieces in the mould, a new era in chemical glassware began, thanks to those products in boro-silicate that would have satisfied the dreams of the masters alchemists of the seventeenth century to have all, or almost all the laboratory instruments made of glass[3].

distillation_8

Frosted cones - Bowl or modern balloon

The Balloon. What once was known in Italian as boccia or bozza (bowl[4]) is now called pallone (eng. Balloon) and presents the same neck with a latest addition of a frosted cone and cap.

The urinale, the ursale, with its large neck, has this name for a good reason; it comes handy in the distillation of human dew and storm water, it helps to retrieve the final dregs. On the other hand these dregs might be collected when they are still damp, and left to dry on a Pyrex plate and then dried, on the same plate. The heat-resistant plate reminds us that they need to be slowly calcinated. In ancient times, when there was not a boro-silicate glass the zucker glas was used, that is, the glass used to build fruit bowls, very thick sugar bowls or exhibitors of candy.

distillation_9

The retort is an alembic in one piece that distills heavy substances, oily or difficult to pass through: it's a ball that bends and twists on itself producing a long beak that is more narrow towards the end, where the distillate is dripping.

distillation_9

The modern version and the original sketch of the flask designed by Dr. Erlenmeyer

The vesica is an oblong copper cylinder, often tinned, that facilitates the rising of the vapours and let them reach the helm without get restricted in the neck. The distillate descends due to refrigeration. Today the Erlenmeyer flasks are commonly used, and on these is placed a Liebig distiller; in the past a helm was placed on the tin coated copper vesica, that was coated so that no substances would suffer any change, e.g. a vitriolation, thus becoming poisonous.

The phial is very similar but made of another material, earthenware, stoneware or glass, and is also useful for aqueous distillates, vaporous, therefore airy, light. Good to distill fruit and spirits. Even this instrument could be replaced today by an Erlenmeyer flask and mounting a boron-silicate glass helm or, as already said, a Liebig distiller.

The cucurbit, as we mention before, has a long and wide neck and it gets attached to the helm.

In ancient times to let the substance circulate, and be processed ascendind and descending inside the flask, rather than distilled, they used the long neck flask, the matraccio, as it is still known today: its lower part is flatter but retains the shape of the neck as in the old times, very long and narrow completed with cone and frosted glass-stopper.

In the Anglo-Saxon world it is known as Florentine vase, florentine flask or a similar name, and in some variables as volumetric flask, in case it has a ground-glass stopper.

distillation_10

Volumetric flask with a ground-glass stopper - Florentine flask

To circulate, for the so-called rotations, or process the substance in one flask, today we use circulators, namely a set of several pieces of glassware joint together to allow the communication between the various parts, and also to slightly heat, expand and cool the substances.

For the same purpose, in the past, a retort and a container of the same shape and size were placed, well joined together and both heated; They were the so-called vasi di ritorno, return vessels; but also "blind" pieces were used with only one opening from which to fill and empty, already shaped for this purpose: they were the gemelli, the twins, two balloons joined together who have on the side of both helms, a beak descending (per descenso) in each other's body, and the “pelican”, or the “crane” a single balloon with a beak descending down inside itself.

Techniques and adjustments

We shall now put together the themes that will guide our choices.

We may find in whatever needs to be distilled more or less delicate principles that risk to be dispersed during the distillation as well as the fact already observed, that the distilled material, can rise more or less, depending on its weight.

It is important that the distillation apparatus can absorb air without losing vapour: if the apparatus was tightly closed, the distillation would be very slow and risky in case of flammable materials. Nowadays, with air tight frosted cones and plugs, it seems necessary to put a small opening for air where the apparatus is already in contact with the receiver; In the old times the problem was quite the opposite: to be able to close all the possible cracks in the apparatus.

There are indeed two systems used to deal with the weight of the substance: on one hand the distillation “per ascenso”, by letting the substance rise, on the other hand the many adjustments to the pieces we already have; if the retort, through which we can distill heavy or oily substances in the best way, is not available, the balloon or the rostrums can be tilted, distilling per descenso, by letting the distilled substance go down.

Considering the heat, the barometric pressure, and the lunation, we can see the quantity that gets distilled, the time needed and the quality of the distilled substance; sorry just after watching some distillations you will know what to do.

In the distillation per ascenso (by elevation), we can stack various glasses before reaching the helm and the rostrum, or a long neck cucurbit with distillation per descenso (by descent) or by the side we can tilt the balloon we are heating up, provided it is enough empty.

Compared to the distillation by the side, the distillation per descenso is for heavier substances; as it is the distillation by retort.

distillation_11

If you have a retort and the substance is really oily or heavy is better not to have in the retort a big "pocket" between the balloon and the nose: in the retort above, there is no pocket or a corner. The retort in the image of three pages ago, has both the "pocket" and the corner; here below there are the separated hitch.

distillation_12

Distillation per ascenso: is used mainly for alcohol.

Distillation by the side: dry wood, bones, horns, blood, gums, resins and tears, honey and sugar, and salts like vitriol, alum, saltpetre, common salt.

Distillation per descenso: is useful for the oils and in this case the retort can be used as well. The per-descenso apparatus can be useful, in the urine process when you need to sublimate its salts in the beak/rostrum, for example, of a liebig distiller.

All the distillers apparatus can be refrigerated on the rostrum (Liebig condenser) some inches after the curve, since we need for the steam to easily overcome the curve; another way to cool, then be condensed; the distillation is with ice around the receiver. The best solution - specially in this case - would be to use an ice maker machine and then, to cool the part around the rostrum, a motor for aquarium that send the icy waters to circulate in the coolant around the rostrum. An easier way is using PVC iced bottles immersed in a bucket full of cold water; It would be better than wasting the tap water.

Beware. An important aspect of Alcohol distillation

When we distill alcohol we must consider that the first drops that come out are named “the head of distillation” and they must be removed. The head contains the toxic substances; they can be detected by the smell that seems of chemical solvents. Indeed acetone starts to evaporate as soon as the distilling alcohol reaches 56 °C, the methanol at about 65 °C, and we must get rid of them at every distillation. In the next distillation, if you go on coobate, it is good to let few drops pass through and throw them, they can be recognised by their offensive smell. Nobody tells that; I wander about the quality of the ancient spirits…

distilla 13

The modern answer to distillation need: the Liebig distiller

distilla 17

Sketch taken from a notebook by Leonardo da Vinci

distilla 12

Codex Atlanticus, folio 216 r - Improved Alembic, study by Leonardo da Vinci

distilla 15

Keck clips for laboratory glassware


1. Sometimes imprecisely defined alambicco - alembic that actually means the whole device.

2. This is the ”lute of knowledge”, as explained by Isaac Newton in his notebooks: lutum sapientiae cum mastice preparandum. Raymund in Th. Ch. v. 4 p. 181. cum gypso et albugine ovi vel farina et albumine ovi Arnold in Th. Ch. v. 4. p. 550. et in Arte Aurif. part. 3. p. 160. Ex flore farinae albuminibus ovorum distemperato. Raymund in Th. Ch. v. 4. p. 141. Ex cera Anonym. in v. 3 Th. Ch. p. 13. cum olibano vel mastice molli vel viva calce et Ovorum albumine. Raymund. de quintessentia p. 25. cum bolo armeni, calce viva claro ovorum et pulvere vitri aequaliter mixtis Plinius Philos in Th. Ch. vol 6 p. 478. Morien. Rom. p. 33. University of Indiana biblioteque

3. The common glass is made by quartz sand, a fluxing agent to lower the melting point of the crystal and a stabilizer: the flux is soda (Na2CO3) or potash (K2CO3), the stabilizer is lime (CaCO3). Please notice that here there are at least two important alchemic ingredients, that are quartz sand (flint) and lime.

4. Again: bowl here means not a cup but a pot.

Letto 1092 volte

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    The twenties, Nice, France... Gold! This article comes from a French review that dates from 1927, written by Andre Ibels for the Nouveau Journal de Nice At the end of the five chapters of the article you will find the protestation by a Professor of Engineering at the Conservatoire des Arts et Metiers in Paris, that accused the scientists of her time of being cowardly.

    We took the article from the Adam Mc Lean website1, probably the best site of alchemy ever. The article was written by Mark House, an American researcher in alchemy, who in the next issue of NitroGeno will write a commentary about this text and the experiments that took place.

    How i succeeded in making gold according to the process of mr. Jollivet Castelot - December 1925
    By A. Ballandras

    Dosage of Gold obtained by the second method.

    The residue, which had been obtained by a mixture of:

    • Silver 10 grams
    • Tin 3 grams
    • Arsenic sulphide 3 grams
    • Antimony sulphide 3 grams

    was crushed as much as possible and subdued (read: subjected) to a treatment of pure chloric acid like in the first method. [Here is a reference to a first method - not presented here - the above being the second method presented by Ballandras from a text, the name and size of which is unknown to me.] However, to completely eliminate the silver and the tin employer, I scrupled to begin the indicated treatments, that is to say that the powder which was obtained having been subdued first to the action of azotic acid then washed with distillated water, then subdued to the action of chloric acid, then once more washed with distillated water, and these different operations were begun once more with another portion of pure azotic acid, and another portion of pure chloric acid after having carefully washed the insoluble residue was subdued to the prolonged action of aqua regalis following:

    Chloric acid - 15 parts/ Azotic acid - 4-5 parts.

    It must be noted that this thing happened during the ebullition (bubbling; boiling) The washed residue contained the slighter part of gold, this thing would be found dissolved in the last liquor, which I obtained. After 18 hours of digestion at the temperature of about 25 degrees, I subdued the mixture to ebullition during 3 hours. After refrigeration, I filtered this on wool of glass and I looked to see if parts were not drawn along in suspense. Finding nothing I proceeded with an analysis of the liquor which I obtained. For that month I made two parts strictly equal of the liquor, the first being destined to qualitative analysis, the other quantitative.

    A) Qualitative Analysis: Assay of usual reagents:

    • Chloride of Tin - Rose colored precipitate
    • Pure Soda in solution - Voluminous yellow reddish precipitate
    • Sulfate of Iron - During ebullition, metallic precipitate, greenish black very dense spangles.

    B) Quantitative Analysis:

    The second part of the liquor destined to undergo quantitative analysis was treated by H2S when the most important part of chloric and azotic acids were driven out by a prolonged ebullition.

    This time the liquor was slightly acid and had a weak smell of chlorine. I called H2S into action; about 20 minutes long. The black precipitate which I obtained was received by a filter paper carefully washed first with well distillated water, then with hot water and at last with chloric acid. After drying in the vapor-bath, the precipitate was put in a capsule of porcelain and heated in a mould at about 850 degrees, so as to destroy the sulphides precipitated with gold i.e., the arsenic and the antimony. These were naturally decomposed by the temperature of 850 degrees to which it had been subdued during two hours. The quantity of gold obtained was 0.238 grains. The half of the liquor having served for the dissolution having been turned to good use for the qualitative analysis it followed that the whole quantity of gold contained in the original liquor should be equal to double the quantity obtained. i.e., 0.476 grains of gold per 10 grams of silver employed, yield then was 0.476 grains of gold per gram silver. {I must point out that the obtaining of gold is not a mathematical regularity, that is to say, the purport (proportion) of residue changes according to the conditions of heating.}

    old drugstore

    2) Dry method

    I acted on 22 grains of chemically pure silver supplied by Messrs. Poulenc of Paris and on 3.5 grains of chemically pure orpiment supplied by the Pharmacie Central of Paris. The mixture was heated to about 1600 C in a metal smelting furnace for about ¾ hour. The residue obtained was again melted for an hour with the addition of orpiment, after having been hammered for half an hour and re-melted with the addition of small quantities of orpiment every 10 minutes, it was withdrawn. After cooling and the addition of chemically pure antimony sulphide, it was again put back into the furnace, small quantities of orpiment being thrown in every 5 minutes. The residue obtained had a dark metallic tint, after hammering it became slightly golden.

    Analysis of the Residue

    The residue dissolved in chemically pure 36 degree HNO3 first cold and then hot, gave an abundant pulverulent deposit. This deposit after being washed and treated with HN3 to dissolve the arsenic and antimony salts was completely dissolved in aqua regia. The liquor after being chlorinated and filtered was subjected to the reagents of Platinum and gold.

    Mr. Andre Vandenberghe who was acting as preparator for this experiment, had thought that in accordance with the law of evolution of matter, the transmutation of bodies into gold should be preceded or accompanied by their transmutation into platinum. According to Mendeleiev’s progression, we have Pt - 195.2 and Au - 197.2

    The reactions of gold were quite characteristic; the reactions of platinum also seemed to reveal its presence. The quantity of gold obtained in this experiment was estimated at about one gram. I emit the hypothesis that the arsenic acts as a catalyzer and the sulphur as a ferment in this transmutation.

    Jollivet Castelot, Douai, December 1925

    A recent experiment in transmutation

    By M. Jollivet Castelot

    All my research work on transmutation since 1908 has started from the fact that gold is found in nature associated with antimony and arsenic sulphides as well as with Tellurium which is considered as the mineralizer of gold. I therefore considered it logical to introduce Tellurium into the artificial combination of silver and arsenic and antimony sulphides that I make. The following is an account of one of my recent experiments:bI prepared a mixture composed of 6 grams of chemically pure silver, 1 gram of native orpiment (Arsenic trisulphide A52S3) free from gold, 1 gram of chemically pure antimony sulphide, and 2 grams of chemically pure Tellurium. I added pure silica to the usual fluxes. This mixture was heated in the furnace in the usual way for one hour at a temperature of 1100 C (approximately) [note: parenthesis are not mine AMWH].

    The residue obtained was of a blackish grey color with violet reflections. It weighed 6.420 grains. When subjected to the action of nitric acid, the residue was attacked with difficulty and greenish metallic particles became detached. The solution was then decanted and a greenish-yellow residue remained which was kept at the boiling point in nitric acid for several hours, after decanting off the liquor once again, the residue, which had not changed, was washed, treated with ammonia and then subjected to the action of aqua regia in which it was entirely dissolved after boiling for several hours.

    The solution after being chlorinated and then subjected to the reagents of gold, gave the following:

    • Potassium Ferrocyanide - greenish brown coloration.
    • Tin Protochloride + Tin Bichloride - a yellow bronze coloration and then a metallic deposit of the same shade.
    • Ammonia - coloration and precipitate identical with the preceding one and which became transformed into a yellow deposit of fulminating gold at the end of a few hours.
    • Formol - light yellowish black metallic precipitate.
    • Peroxide of Hydrogen - light very finely divided brownish black precipitate.
    • Oxalic acid - yellowish black precipitate.
    • Ferrous Sulphate - golden yellow metallic precipitate.
    • Caustic Potash - a fairly abundant golden yellow metallic precipitate at the end of a few hours.

    The presence of gold was therefore very distinctly shown and a remarkable feature was that the metal obtained possessed the yellow bronze color of gold telluride and of native silver. I had therefore produced a bronze colored gold in my laboratory by artificial means thanks to the intervention of the Tellurium.

    “A certain amount of gold was certainly lost in this test as in all my previous tests, for it is known that arsenic, antimony and Tellurium entrain gold in their fusion and their volatilization. In order to obviate this disadvantage, I had thought of making the vapors of arsenic and antimony sulphides and of Tellurium act on the silver in fusion in a closed vessel by means of a special device, but I have been forced to give up this scheme for the time being on account of the difficulties met with for the construction of this apparatus, the cost of which would be very high. I consider it certain that if the vapors were allowed to bubble through the melted silver, a much higher yield of gold would be obtained than that I have obtained hitherto by an imperfect and too rapid contact of the bodies in presence; while it is undoubtedly necessary to make them react on one another in the state of vapor in a closed vessel.” Jollivet Castelot, Douai, April 24th, 1926

    The chemical manufacture of gold account of one of my last experiments in the transmutation of silver into gold

    As a sequel to my previous work on the artificial synthesis of gold, I have introduced Tin into these new tests as it is also often associated with gold in nature. The following is a description of this new process, thanks to which the percentage of gold obtained destroys all the objections that are raised with regard to impurities.

    I made an intimate mixture of 6 grams of chemically pure silver of which the purity was tested by a professional chemist, the Head of the laboratory of one of the most important Works of the region. 2 Grams of antimony sulphide, 1 gram of orpiment, and 1 gram of Tin; all these bodies were obtained from the Establishment Poulenc of Paris and were chemically pure. I added the usual fluxes and then heated the whole in a crucible in the furnace to about 1100 C fort2 about 1 hour, twice adding a small quantity of antimony sulphide.

    The residue obtained was treated for a long period in pure 36 degree nitric acid, first cold and then at the boiling point.

    The insoluble residue was next washed with distilled water, treated with ammonia, washed again and finally treated for a long period with boiling aqua regia. The liquor when filtered and subjected to the reagents of gold showed the presence of this metal in the form of deposits3 which maybe estimated at 0.05 grains in all, which is very high considering the 6 grams of silver employed.

    With Oxalic acid, the solution turned violet and gave an abundant black pulverulent precipitate.

    With Hydrogen Peroxide, a very finely divided precipitate of gold.

    With Formic Aldehyde, a brown precipitate of gold.

    With Tin Protochloride, an intense violet pink coloration.

    The addition of Tin to the other bodies has certainly facilitated the reactions of the gold and increased the yield of this metal which can be manufactured artificially by my process.

    It would be easy to show that, given the respective prices of gold and of the other substances that are used in my process to produce it, a profit could be obtained if the process were worked industrially; all the more so as the greater part of the silver employed can be recovered at each test.

    I believe I now hold the key to the regular and even industrial manufacture of gold. But the industrial question is voluntarily put aside from my thoughts, for my only object is the search for pure scientific truth.
    Jolivet Castelot, Douai, April 15th, 1927

    Table of reactions

    “GOLD”

    • C2H2O4 - Abundant deposit of metallic gold.
    • H2O2 (basic) - Brown precipitate.
    • K4 Fe Cy6 . 3H2O - Green coloration.
    • Na2CO3 (in ebullition) - Brownish precipitate.
    • “PLATINUM & GOLD”
    • NH3 - Reddish yellow precipitate (Au); topped by a yellow precipitate (Pt).
    • KOH - Reddish yellow precipitate (Au); topped by a yellow precipitate (Pt).
    • SnCL2.2H2O - Solution colored brown with reactions of platinum salts and deposit of black powder.
    • KI - Solution becomes reddish followed by a discharge of iodine and a brown precipitate (Platinum iodide).

    Extracts from the press

    “It must be admitted that it is extraordinary and incomprehensible that France for the past ten years has refused to take an interest in the experiments of a rich and universally respected scientist who has given proofs of his worth, even after the conclusive experiments carried out by an official chemist, Mr Ballandras of Lyons.”
    Andre Ibels, La Razon, June 8, 1927

    It is unjust, gentlemen, that a scientist of the value of Mr. Jollivet Castelot should be held in suspicion at the very moment when he is losing his sight through overwork. To continue his work, however embarrassing it may be to yours, is a sacred duty.”
    Declaration by Mademoiselle M.L. of Paris. Professor of Engineering at the Conservatoire des Arts et Metiers, Paris, at the Chemical Congress in Paris. October 1927

    “Oh! it is not that Mr. Jollivet Castelot has not attempted to make his invention known in France, on the contrary, he has written leaflets and books and has founded reviews for this purpose... Not only was he not taken seriously, but he was also a butt to the sarcasm and even to the insults of the official scientists in general and of the Nobelist Perrin in particular. The Acedemie des Sciences itself - as usual - refused to record his communication.”
    Andre Ibels, Nouveau Journal de Nice, October 16, 1927

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